• Bulletin of the Korean Chemical Society
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• 제34권12호
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• pp.3695-3702
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• 2013

A nickel(II) complex $[Ni(H_2biim)_2(H_2O)_2](ClO_4)_2{\cdot}H_2O$ (1) of biimidazole ligand has been synthesized and characterized (Where $H_2biim$ = 2,2'-biimidazole). The single crystal X-ray diffraction of the complex shows a dimeric structure with six coordinated psudo-octahedral geometry. The cyclic voltammograms of complex exhibited one quasireversible reduction wave ($E_{pc}=-0.61V$) and an irreversible oxidation wave ($E_{pa}=1.28V$) in DMF solution. The interaction of the complex with Calf-Thymus DNA (CT-DNA) has been investigated by absorption and fluorescence spectroscopy. The complex is an avid DNA binder with a binding constant value of $1.03{\times}10^5M^{-1}$. The results suggest that the nickel(II) complex bind to CT-DNA via intercalative mode and can quench the fluorescence intensity of EB bind to CT-DNA with $K_{app}$ value of $3.2{\times}10^5M^{-1}$. The complex also shown efficient oxidative cleavage of supercoiled pBR322 DNA in the presence of hydrogen peroxide as oxidizing agent. The DNA cleavage by complex in presence of quenchers; viz. DMSO, KI, $NaN_3$ and EDTA reveals that hydroxyl radical or singlet oxygen mechanism is involved. The complex showed invitro antimicrobial activity against four bacteria and two fungi. The antimicrobial activity was nearer to that of standard drugs and greater than that of the free ligand.

• Bulletin of the Korean Chemical Society
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• 제34권12호
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• pp.3635-3640
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• 2013

We prepared Ni and Pd-modified $TiO_2@SiO_2$ core-shell nanostructures and then analyzed them by scanning electron microscopy, optical microscopy, X-ray diffraction crystallography, FT-IR and UV-Visible absorption spectroscopy. In addition, their CO oxidation performance was tested by temperature-programmed mass spectrometry. The CO oxidation activity showed an order of Ni-$TiO_2@SiO_2$ ($900^{\circ}C$) < Ni-$TiO_2@SiO_2$ ($90^{\circ}C$) < Ni-$TiO_2@SiO_2$ ($450^{\circ}C$) in the first CO oxidation run, and greatly improved activity in the same order in the second run. The $T_{10%}$ (the temperature at 10% CO conversion) corresponds to the CO oxidation rate of $2.8{\times}10^{-5}$ molCO $g{_{cat}}^{-1}s^{-1}$. For Ni-$TiO_2@SiO_2$ ($450^{\circ}C$), the $T_{10%}$ was observed at $365^{\circ}C$ in the first run and at $335^{\circ}C$ in the second run. For the Pd-$TiO_2@SiO_2$ ($450^{\circ}C$), the $T_{10%}$ was observed at a much lower temperature of $263^{\circ}C$ in the first CO oxidation run, and at $247^{\circ}C$ in the second run. The CO oxidation activities of transition metal modified $TiO_2@SiO_2$ core-shell nanostructures presented herein provide new insights that will be useful in developing catalysts for various environments.

• Journal of Magnetics
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• 제20권3호
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• pp.229-240
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• 2015

In this study, nanocrystalline ferrite powders with the composition $Ni_{0.5}Zn_{0.5}Fe_2O_4$ were prepared by the autocombustion method. The obtained powders were sintered at $800^{\circ}C$, $900^{\circ}C$ and $1,000^{\circ}C$ for 4 h in air atmosphere. The as-prepared and the sintered powders were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, and magnetization studies. An increase in the crystallite size and a slight decrease in the lattice constant with sintering temperature were observed, whereas microstrain was observed to be negative for all the samples. Two significant absorption bands in the wave number range of the $400cm^{-1}$ to $600cm^{-1}$ have been observed in the FT-IR spectra for all samples which is the distinctive feature of the spinel ferrites. The force constants were found to vary with sintering temperature, suggesting a cation redistribution and modification in the unit cell of the spinel. The M-H loops indicate smaller coercivity, which is the typical nature of the soft ferrites. The observed variation in the saturation magnetization and coercivity with sintering temperature has been attributed to the role of surface, inhomogeneous cation distribution, and increase in the crystallite size.

• 한국광물학회지
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• 제2권1호
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• pp.26-36
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• 1989

Clinopyroxene in the Geodo mine belongs to diopside-hedenbergite series. It is widely distributed throughout the mine area together with garnet and is also closely related with Fe-mineralization. Clinopyroxenes in the Geodo mine including two samples from the sangdong and Ulchin Mines are studied using polarized microscope, EPMA, XRD, and IR spectroscopy for occurrence, chemistry, structure, and crystal chemistry. Especially, variations in unit-cell parameters are examined in relation with the substitution scheme between Fe and Mg cations. Clinopyroxenes in the Geodo mine occur in both endoskarn and exoskarn zone. It is mostly anhedral to subhedral with fine- to medium-grained in texture, but some have bigger crystals of short prismatic or columnar habits. Clinopyroxene occurs as monomineralic or is associated with mostly garnet and sometimes with actinolite, magnetite, epidote, and chlorite. Chemical analysis reveals that the Geodo clinopyroxene is diopsidic in composition (Di: 65-96%). This fact is in good contrast with garnet chemistry showing mostly andraditic (An: 41-82%). Especially, clinopyroxene coexisting with magnetite belongs to nearly end member diopside (Di: 97-99%). Thus, diopside-andradite pair indicates that Geodo skarns were formed under the reduced environment. X-ray diffraction analysis shows unit-cell parameters vary with increase of Fe contents: a = 9.765-9.838$\AA$, b = 8.943-9.020$\AA$, c= 5.240-5.253$\AA$.$\beta$ = 105.70-104.83$^{\circ}$, and V =440.64-448.19$\AA$3. It is noted from the least square regression that a, b and V increase linearly with increase of Fe content, while $\beta$ slightly decreases and c remains nearly unchanged as change in Fe content. These trends are to difference between synthetic and natural clinopyroxenes. This fact is also recognized in IR spectra which show a slight shift of several absorption bands toward lower wavenumber region with increasing Fe content.

• The Journal of Advanced Prosthodontics
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• 제6권3호
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• pp.207-214
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• 2014

PURPOSE. This study characterized the synthesis of a modified PMMA (Polymethyl methacrylate) denture acrylic loading platinum nanoparticles (PtN) and assessed its bacterial inhibitory efficacy to produce novel antimicrobial denture base material. MATERIALS AND METHODS. Polymerized PMMA denture acrylic disc ($20mm{\times}2mm$) specimens containing 0 (control), 10, 50, 100 and 200 mg/L of PtN were fabricated respectively. The obtained platinum-PMMA nanocomposite (PtNC) was characterized by TEM (transmission electron microscopy), SEM/EDX (scanning electron microscope/energy dispersive X-ray spectroscopy), thermogravimetric and atomic absorption spectrophotometer analysis. In antimicrobial assay, specimens were placed on the cell culture plate, and $100{\mu}L$ of microbial suspensions of S. mutans (Streptococcus mutans) and S. sobrinus (Streptococcus sobrinus) were inoculated then incubated at $37^{\circ}C$ for 24 hours. The bacterial attachment was tested by FACS (fluorescence-activated cell sorting) analysis after staining with fluorescent probe. RESULTS. PtN were successfully loaded and uniformly immobilized into PMMA denture acrylic with a proper thermal stability and similar surface morphology as compared to control. PtNC expressed significant bacterial anti-adherent effect rather than bactericidal effect above 50 mg/L PtN loaded when compared to pristine PMMA (P=.01) with no or extremely small amounts of Pt ion eluted. CONCLUSION. This is the first report on the synthesis and its antibacterial activity of Pt-PMMA nanocomposite. PMMA denture acrylic loading PtN could be a possible intrinsic antimicrobial denture material with proper mechanical characteristics, meeting those specified for denture bases. For clinical application, future studies including biocompatibility, color stability and warranting the long-term effect were still required.

• 한국재료학회지
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• 제27권4호
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• pp.206-210
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• 2017

In this study, an ${\alpha}-Fe_2O_3$ (hematite) coated porcelain plate was sintered in a temperature range from $1100^{\circ}C$ to $1250^{\circ}C$ using ferrous sulfate. The specimens were investigated by X-ray diffractometer (XRD), scanning electron microscopy (FE-SEM), energy dispersive spectroscopy (EDS), and UV-visible spectrophotometer. It was confirmed that ${\alpha}-Fe_2O_3$ (hematite) was densely fused to the surface at several tens of ${\mu}m$, the ${\alpha}-Fe_2O_3$ (hematite) was in the form of thin platelet and polyhedra, and no other compounds appeared in the sintering process. In the specimen coated with ${\alpha}-Fe_2O_3$ (hematite), the reflectance spectra show a red absorption band of 560-650 nm. The $L^*$ value decreased from 53.18 to 46.94 with the firing temperature. The values of $a^*$ and $b^*$ were at 19.03 and 15.25 at $1100^{\circ}C$ and gradually decreased with increasing temperature; these values decreased rapidly at $1250^{\circ}C$ to 11.54 and 7.98, respectively. It is considered that the new phases are formed by the phase transition of the porcelain plate (clay), and thus the $a^*$ and $b^*$ values are greatly influenced.

• 한국자기학회지
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• 제16권1호
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• pp.14-17
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• 2006

졸겔법을 이용하여 $AIFeO_3$ 단일상을 제조하였으며, 그 결정학적 및 자기적 특성을 X선 회절법(XRD), 진동 시료 자화율 측정법(VSM), 뫼스바우어 분광법으로 연구하였다. 결정구조는 공간군이 $Pna2_1$ orthorhombic 구조로 분석되었으며, 격자 상수는 각각 $a_0=4.983\;{\AA},\;b_0=8.554\;{\AA},\;c_0=9.239\;{\AA}$임을 알 수 있었다. VSM을 이용하여 65K에서부터 상온까지 여러 온도 구간에서 자기이력곡선을 측정하였으며, 강자성 특성과 함께 저온영역에서 자기 이력 곡선의 비대칭성이 관측되었다. 온도에 따른 자기모멘트 측정 결과로부터 자기전이온도는 250k로 결정하였다. 뫼스바우어 스펙트럼은 4.2K에서부터 상온까지의 온도 영역에서 측정하였으며, 분석 결과 상온에서 이성질체 이동치는 0.32mm/s로 철의 이온상태가 ferric임을 확인할 수 있었다. 온도변화에 따라 측정된 뫼스바우어 스펙트럼 분석은 온도에 따라 선폭이 증가함이 관측되었는데, 이러한 흡수선의 비대칭적 선폭 증가는 1개의 사면체자리와 3개의 팔면체 자리의 Fe이온 분포와 각 부격자간 자기이방성 에너지 차이에 따른 결과로 해석된다.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2013년도 제44회 동계 정기학술대회 초록집
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• pp.552-552
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• 2013

In our study we consider Al2O3 ceramic substrates for Plasma Surface Treatments in order to improve deposited diamond surface and increase diamond deposition rate by applying DBD (Dielectric Barrier Dischrge) system. Because Plasma Surface Treatments was used as a modification method of material surface properties like surface free energy, wettability, and adhesion. By applying Plasma Surface Treatments diamond films are deposited on the Al2O3 ceramic substrates. DC Arc Plasmatron with mathane and hydrogen gases is used. Deposited diamond films are investigated by SEM (Scanning Electron Microscopy), AFM (Atomic Force Microscopy) and XRD (X-ray Diffractometer). Then the C-H stretching of synthetic diamond films by FTIR (Fourier Transform Infrared Spectroscopy) is studied. As a result, nanocrystalline diamond films were identified by using SEM and diamond properties in XRD peaks at (111, $43.8{\Box}$, (220, $75.3{\Box}$ and (311, $90.4{\Box}$ were shown. Absorption peaks in FTIR spectrum, caused by CHx sp3 bond stretching of CVD diamond films, were identified as well. Finally, we improved such parameters as depostion rate ($2.3{\mu}m$/h), diamond surface uniformity, and impurities level by applying Plasma Surface Treatments. These experimental results show the importance of Plasma Surface Treatments for diamond deposition by a plasma source.

• Bulletin of the Korean Chemical Society
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• 제26권7호
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• pp.1044-1050
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• 2005

The reaction of cis-[Cr([14]-decane)($OH_2)_2]^+$ ([14]-decane = rac-5,5,7,12,12,14-hexamethyl-1,4,8,11-teraazacyclotetradecane) with auxiliary ligands {$L_a$ = isothiocyanate ($NCS^-$), azide ($N3^-$) or chloroacetate(caa)} leads to a new cis-[Cr([14]-decane)($NCS)_2]ClO_4{\cdot}H_2O$ (1), cis-[Cr([14]-decane)($N_3)_2]ClO_4$ (2) or cis-[Cr([14]-decane)($caa)_2]ClO_4$ (3). These complexes have been characterized by a combination of elemental analysis, conductivity, IR and Vis spectroscopy, mass spectrometry, and X-ray crystallography. Analysis of the crystal structure of cis-[Cr([14]-decane)($NCS)_2]ClO_4{\cdot}H_2O$ reveals that central chromium(III) has a distorted octahedral coordination environment and two $NCS^-$anions are bonded to the chromium(III) ion via the Ndonor atom in the cis positions. The angle $N_{axial}-Cr-N_{axial}$ deviates by 13$^{\circ}$ from the ideal value of 180$^{\circ}$ for a perfect octahedron. The bond angle N-Cr-N between the Cr(III) ion and the two nitrogen atoms of the isothiocyanate ligands is close to 90$^{\circ}$. The bond lengths of Cr-N between the chromium and $NCS^-$groups are 1.964(5) and 2.000(5) $\AA$. They are shorter than those between chromium and nitrogen atoms of the macrocycle. The IR spectra of 1, 2 and 3 display bands at 2073, 1344 and 1684 $cm^{-1}$ attributed to the $NCS^-$, ${N_3}^-$ and caa groups stretching vibrations, respectively.

• Bulletin of the Korean Chemical Society
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• 제29권9호
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• pp.1711-1716
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• 2008

The reaction of copper(II) chloride with phenyl-N-[(pyridine-2-yl)methylene]methaneamide (ppmma) leads to a new $\mu$ -chloro bridged dimeric [Cu(ppmma)$Cl_2$]$_2$ complex, whereas a reaction of copper(II) bromide with ppmma affords a monomeric Cu(ppmma)$Br_2$ complex. Both complexes have been characterized by X-ray crystallography and electronic absorption spectroscopy. The crystal structural analysis of [Cu(ppmma)$Cl_2$]$_2$ shows that the two Cu(II) atoms are bridged by two chloride ligands, forming a dimeric copper(II) complex and the copper ion has a distorted square-pyramidal geometry ($\tau$ = 0.2). The dimer units are held through a strong intermolecular $\pi-\pi$ interactions between the nearest benzyl rings. On the other hand, Cu(ppmma)Br2 displayed a distorted square planar geometry with two types of strong intermolecular π-π interaction. EPR spectrum of [Cu(ppmma)$Cl_2$]$_2$ in frozen glas s at 77 K revealed an equilibrium between the mononuclear and binuclear species. The magnetic susceptibilities data of [Cu(ppmma)$Cl_2$]$_2$ and Cu(ppmma)$Br_2$ follow the Curie-Weiss law. No significant intermolecular magnetic interactions were examined in both complexes, and magnetic exchange interactions are discussed on the basis of the structural features.